Classifications

• • C—CHEMISTRY; METALLURGY
  • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
  • C12C—BEER; PREPARATION OF BEER BY FERMENTATION; PREPARATION OF MALT FOR MAKING BEER; PREPARATION OF HOPS FOR MAKING BEER
  • C12C7/00—Preparation of wort
  • C12C7/14—Lautering, i.e. clarifying wort
  • C12C7/16—Lautering, i.e. clarifying wort by straining
  • C12C7/165—Lautering, i.e. clarifying wort by straining in mash filters
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
  • B01D67/0002—Organic membrane manufacture
  • B01D67/002—Organic membrane manufacture from melts
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
  • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
  • B01D71/06—Organic material
  • B01D71/24—Rubbers
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
  • B01D71/06—Organic material
  • B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
  • B01D71/80—Block polymers
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2323/00—Details relating to membrane preparation
  • B01D2323/30—Cross-linking
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2325/00—Details relating to properties of membranes
  • B01D2325/24—Mechanical properties, e.g. strength

Definitions

• the invention is in the field of brewing beverages like beer.
• the invention is directed to a mash filter membrane for use in the filtration of mash.
• Mashing is typically a process step in brewing wherein milled grain and water are combined and heated to form and extract the sugars and other components from the grains to form mash, which is a suspension comprising wort and solid, spent grain. To continue the wort further into the brewing process, it needs to be separated from the spent grain in the mash in a mash filtration or lautering process. In large scale breweries, this is typically carried out with a mash filtration unit, such as for instance a mash filtration unit described in EP0674929 and commercially available from Meura S.A., Belgium. Other, similar types of mash filtration units are commercially available from Landaluce S.A., Spain and Lehui, China.
• a mash filtration unit such as for instance a mash filtration unit described in EP0674929 and commercially available from Meura S.A., Belgium.
• Other, similar types of mash filtration units are commercially available from Landaluce S.A.
• mash is led into chambers of a mash filtration unit, between a filter, generally a cloth filter, and a membrane, occasionally also referred to as bladder.
• the membrane is used to apply pressure on the mash such that the wort is pushed through the filter out of the mash.
• the remaining spent grain bed, that is positioned (sandwiched) between the filter and the membrane can optionally be rinsed with hot water, to further extract remaining sugars from the spent grain bed.
• the chambers are opened to release the spent grain bed and the cycle can be repeated with another brew or batch of mash.
• the mash filter membrane is elastic to a certain extent, such that it can be deflated when mash is introduced into the chamber and inflated to apply further pressure (e.g . about maximum 1200 mbar) on the mash.
• Conventional mash filter membranes such as those commercially available from Meura S.A., are associated with a number of drawbacks.
• the membrane After a certain number of brews, the membrane’s structural integrity fails due to breaks or tears such that the membrane must be replaced. This replacement requires undesired downtime of the filtration unit. Moreover, problematically, the frequency of failure of the membrane is relatively unpredictable, meaning that one membrane of a particular type may last longer than another membrane of the same type. This is indicative of a variable rubber composition for each membrane. This unpredictable durability of conventional membrane makes it difficult to schedule maintenance and leads to even more downtime. In addition to tearing or breaking, conventional mash filter membranes tend to form creases or folds over time. Creasing not only influences the structural integrity of the membrane but also hampers the release of the spent grain bed from the opened chambers, as the spent grain bed remains hanging on the creases.
• DE4313103 discloses a membrane filter system and an elastomeric membrane sheet.
• the sheet is consider elastomeric while it is exphcitly disclosed that that a part the sheet is not elastomeric.
• conventional membranes even if having elastomeric properties, may nonetheless contain less than 50% elastomers.
• a diaphragm for a filter press is disclosed. It is described that the diaphragm shows good heat-resistance and thermal aging resistance or chemical resistance vis-a-vis other diaphragms made of rubber. No information on its suitability in mash filtration, let alone its advantages therein are however known from EP0142173. It is an object of the present invention to provide an improved mash filter membrane that does not suffer from one or more of the drawbacks, such as the above, associated with conventional membranes. In particular, it is an object to provide a more durable mash filter membrane than the conventional membranes such that no or less replacements are required.
• the present inventors surprisingly found that this object can be met by providing a mash filter membrane that retains its elasticity for a large number of brews.
• the invention provides a mash filter membrane comprising an elastomeric composition that comprises more than 50 wt% of one or more elastomer, based on the total amount of polymers in the elastomer composition.
• elastomer herein means a polymer having elastic properties and includes natural and synthetic elastomers, which are also referred to as rubbers.
• the elastomer of the present invention comprises synthetic elastomer for good control of its properties.
• Certain conventional mash filter membranes comprise a elastomeric composition that is based on the elastic copolymer ethylene propylene diene monomer (EPDM) and a non-elastic thermoplastic polymer (also referred to as plastic or thermoplastic phase) such a polyethylene (PE) or polypropylene (PP).
• EPDM elastic copolymer ethylene propylene diene monomer
• PE polyethylene
• PP polypropylene
• the composition comprises 50% EPDM and 50% PE. Since the elastic properties of the membrane can mostly be contributed to EPDM, conventional membranes may occasionally be referred to as EPDM membranes, even though the membranes do contain a plastic such as PE.
• the compositions can be regarded as plastics such that obtaining food grade rating according to the regulation set forth by the relevant authorities (e.g. the U.S. Food and Drug Administration, FDA the Dutch Nederlandse Voedsel- enonnaisautoriteit, NVWA) is facilitated.
• the conventional plastics-containing elastomeric composition may be in accordance with EU Regulations (EU) 10/2011 and/or EU Regulations (EU) 282/2008.
• EU EU Regulations
• EU EU Regulations
• the present elastomeric composition comprises as less plastic as possible.
• an elastomeric composition comprising more than 60% in particular shows an improved durability.
• the increase in durability is observable concomitantly with the increase in the amount of the elastomer in the composition.
• the composition comprises preferably more than 80, preferably more than 90, more preferably more than 95, most preferably about 100 wt% of said elastomers, based on the total weight of polymers in the elastomeric composition.
• the elastomeric composition is essentially free of plastic.
• the limited or none-use of plastic in the present elastomeric composition can alternatively, or additionally be expressed as that the elastomeric composition comprises less than 50% of one or more inelastic polymers such as inelastic thermoplastic polymers, preferably less than 25%, more preferably less than 10%, based on the total weight of polymers in the elastomeric composition.
• the inelastic polymers are typically polyolefin homopolymers, such as one or more polymers selected from the group of polyethylene, polypropylene, polystyrene and the like.
• the elastomeric composition is preferably well resistant to an alkahne solution (e.g . a 2% alkaline solution) which can be used for CIP purposes.
• the elastomer comprises preferably EPDM.
• Other suitable elastomers may be one or more selected from the group consisting of EPDM, FKM (according to ASTM D1418 standard - e.g. VitonTM), FFKM (according to ASTM D1418 standard - e.g. KalrezTM), nitrile butadiene rubber (NBR).
• the elastomer preferably comprises a copolymer such as a block-copolymer like triblock copolymers polystyrene- block -polybutadiene-block-polystyrene (SBS), poly styrene -block- polyisobutene-block-polystyrene (SIS).
• the elastomer comprises an olefinic elastomer such as ethylene propylene rubber (EPR), nitrile butadiene rubber (NBR) EPDM, polystyrene-co- polybutadiene rubber (SBR).
• the elastomeric composition may further comprise additives such as fillers like carbon black, curing agents, stabilizers, plasticizer, and the like.
• additives such as fillers like carbon black, curing agents, stabilizers, plasticizer, and the like.
• the elastomeric composition of the present invention is preferably cured or cross-linked by peroxide.
• the membrane consists essentially entirely of the elastomeric composition.
• the membrane may comprise the composition and a layer or patches of another composition, for instance a perfluorated compound (PFC) composition, located on the side of the membrane that is intended to contact the mash.
• PFC perfluorated compound
• the elastomeric composition of the present invention is preferably food grade. This can surprisingly also be attained for the elastomeric composition essentially consisting of EPDM. As such, the inventors found that it is not required for regulatory purposes to include at least 50% plastic in the composition as is the case for conventional elastomeric compositions.
• the elastomeric composition of the present invention can comply with the regulation laid according to EU Directive 95/2001/EC on general product safety, Regulation (EC) N.
• the elastomeric composition of the present invention also meets the requirements laid down in Regulation (EC) N. 2023/2006 Good Manufacturing Practices.
• a further aspect of the invention is a method for the production of the membrane.
• membranes are generally produced by compression molding.
• a drawback of this method is that it allows for a limited control over process parameters. For instance, segregation of the starting materials such as the raw EPDM and raw PE pellets may occur, which will result in a heterogeneous final composition.
• the present inventor found that the infrequent durability of conventional membrane may be contributed to the poor control of the process in the compression molding.
• the membrane of the present invention is preferably prepared by a molding process comprising blending of a melt of the composition, as is for instance carried out in injection molding. It was found that injection molding leads to more narrow distribution of the durability of the membrane.
• the membrane of the present invention is preferably obtainable by molding process comprising blending of a melt of the composition such as injection molding.
• This method was also found particularly suitable for the production of the relatively large sized membranes in accordance with the present invention, which may have a typically one-sided surface area of more than 1, preferably more than 2, more preferably more than 3, even more preferably more than 3.5, most preferably about 3.6 m .
• the elastomeric composition before use of said membrane, has preferably one or more, more preferably all of the following material properties:
• - a tensile strength determined according to ISO 37:2011, type 2, of more than 5, preferably more than 8, more preferably more than 10 MPa, such as about 12 MPa;
• modulus M300 deformation determined according to ISO 37:2011, type 2, of more than 4, preferably more than 4.5, more preferably more than 5 MPa, such as about 8.6 MPa;
• the elastomeric composition is therefore preferably composed in such a way that the material properties vary as little as possible due to usage. It was found that this is particularly the case for the material property compression set, determined after 72 hours at 70 °C according to ISO 815-1:2014, method A, test piece B.
• the compression set can particularly be used as a reliable parameter for determining the durability of the elastomeric composition.
• compression set is indicative for the elasticity of the composition.
• the initial compression set for conventional membranes such as that available from Meura S.A., Belgium (i.e. ca. 40%)
• the compression set of the membrane increases (e.g . to ca. 59% after 4700 brews).
• the compression set of the membrane according to the present invention remains essentially constant over 4700 brews.
• the mash filter membrane of the present invention preferably has a compression set of less than 35%, more preferably less than 25%, before use of said membrane, and/or a
• a further aspect of the present invention is directed to the use of the mash filter membrane or the mash filtration unit in the filtration of mash.
• the invention is directed to a method comprising the filtration of mash using the mash filter membrane or the mash filtration unit comprising said membrane. More specifically, said method comprises applying pressure with the membrane on mash such that wort is pushed through a filter out of the mash.
• a mash filter membrane comprising a elastomeric composition comprising black, peroxide-cured 100% EPDM (based on the total weight of polymers in the composition) was produced by injection molding.
• the membrane had a size of 2 by 1.8 m 2 and the material properties as indicated in Table 1.
• a mash filter membrane of 2 by 1.8 m 2 available from Meura S.A., Belgium, having a composition of 50 wt% EPDM and 50% PE was analyzed before use and the following material properties as indicated in Table 2 were found.
• Example 1 One mash filtration unit commercially available from Meura S.A. was equipped with 138 mash filter membranes as prepared in Example 1. Another mash filtration unit of the same type, was equipped with 138 conventional mash filter membranes are referred to in Comparative example 1. Both mash filtration units were placed in the same room, fed with the same brews (mash) and treated similarly (expect when
• Example 2 The filtrations units of Example 2 were used for filtration during a time period of approximately 90 weeks, wherein 4700 brews were produces for which the mash was filtered.
• the conventional mash filter membranes as referred to in Comparative example 1 had a fail rate of 13% (18 out of 138), while the mash filter membranes of the present invention according to Example 1 had a fail rate of 0% (0 out of 138).

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• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Organic Chemistry (AREA)
• Biochemistry (AREA)
• Wood Science & Technology (AREA)
• Bioinformatics & Cheminformatics (AREA)
• General Engineering & Computer Science (AREA)
• General Health & Medical Sciences (AREA)
• Genetics & Genomics (AREA)
• Health & Medical Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Zoology (AREA)
• Food Science & Technology (AREA)
• Manufacturing & Machinery (AREA)
• Separation Using Semi-Permeable Membranes (AREA)
• Manufacture Of Macromolecular Shaped Articles (AREA)
• Compositions Of Macromolecular Compounds (AREA)
• Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
• Filtering Materials (AREA)

Priority Applications (13)

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Citations (6)

Family Cites Families (6)

• 2018
  • 2018-08-29 EP EP18191554.7A patent/EP3617301A1/en not_active Withdrawn
• 2019
  • 2019-08-29 EP EP19783142.3A patent/EP3844256B1/en active Active
  • 2019-08-29 WO PCT/NL2019/050553 patent/WO2020046122A1/en unknown
  • 2019-08-29 MX MX2021001899A patent/MX2021001899A/es unknown
  • 2019-08-29 CN CN201980048605.9A patent/CN112469808B/zh active Active
  • 2019-08-29 ES ES19783142T patent/ES2955204T3/es active Active
  • 2019-08-29 BR BR112021003669A patent/BR112021003669A8/pt unknown
  • 2019-08-29 CN CN202410641024.9A patent/CN118416718A/zh active Pending
  • 2019-08-29 PL PL19783142.3T patent/PL3844256T3/pl unknown
  • 2019-08-29 CA CA3107615A patent/CA3107615C/en active Active
  • 2019-08-29 AU AU2019327293A patent/AU2019327293A1/en active Pending
  • 2019-08-29 JP JP2021510224A patent/JP2021536349A/ja active Pending
  • 2019-08-29 US US17/261,619 patent/US20210261893A1/en active Pending
  • 2019-08-29 DK DK19783142.3T patent/DK3844256T3/da active
• 2021
  • 2021-02-16 MX MX2024006247A patent/MX2024006247A/es unknown
• 2024
  • 2024-04-18 JP JP2024067525A patent/JP2024097793A/ja active Pending

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